Determination of low-level ink photoinitiator residues in packaged milk by solid-phase extraction and LC-ESI/MS/MS using triple-quadrupole mass analyzer

Abstract

A confirmatory and quantitative method based on liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) has been developed for simultaneous determination of seven photoinitiator residues: benzophenone, (1-hydroxycyclohexyl)phenylketone (Irgacure 184), isopropylthioxanthone (ITX), 2-ethylhexyl-(4-dimethylamino)benzoate (EHA or EHDAB), 2-methyl-1-[4-(methylthio)phenyl]-2-(4-morpholinyl)-1-propanone (Irgacure 907), (2,4,6-trimethylbenzoyl)diphenylphosphine oxide (TPO) and 2-benzyl-2-(dimethylamino)-1-(4-morpholinophenyl)-1-butanone (Irgacure 369) in packaged milk and related packaging materials. Residues of photoinitiators were extracted from milk using acetonitrile, and further enriched and purified on HLB solid-phase extraction cartridges prior to being analyzed by LC-ESI/MS/MS with selected reaction monitoring mode, while photoinitiators in packaging materials were extracted using the same solvent. Satisfactory recovery (from 80 to 111%), intra- and inter-day precision (below 12%), and low limits of quantification (from 0.1 to 5.0 microg kg(-1)) were evaluated from spiked samples at three concentration levels (5.0, 10.0 and 25.0 microg kg(-1) for Irgacure 184 and 2.5, 5.0 and 25.0 microg kg(-1) for others). These excellent validation data suggested the possibility of using the LC-ESI/MS/MS method for simultaneous determination of low-level photoinitiator residues migrating from printed food-packaging materials into milk. The method has been successfully applied to the analysis of real samples of different fat contents ranging from 8 to 30 g L(-1). The photoinitiator residues were revealed to be higher in milk with higher fat content and the most important contaminations were benzophenone and ITX in concentration ranges of 2.84-18.35 and 0.83-8.87 microg kg(-1), respectively.

Evaluation of the migration of 15 photo-initiators from cardboard packaging into Tenax®using ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

“…A few methods based on LC in combination with UV detection (Papilloud et al 2002;Sanches-Silva et al 2008a, 2008b, 2009 or even fluorescence detection have also been reported (Morlock & Schwak 2006;Sagratini et al 2008). However, LC-MS/MS has gained popularity (Sagratini et al 2006;Bagnati et al 2007;Gil-Vergara et al 2007;Sun et al 2007;Allegrone et al 2008;Gallart-Ayala et al 2008, 2011Sanches-Silva et al 2008;Shen et al 2009). A comparison between GC and LC has shown, however, that both techniques are adequate: LC gives a lower LOQ while the repeatability is comparable (Gil-Vergara et al 2007).…”

Method for analysis of 68 organic contaminants in food contact paper using gas and liquid chromatography coupled with tandem mass spectrometry

“…GCeMS has been frequently used for the analysis of phthalates (Bononi & Tateo, 2009;Zhang et al, 2008) and PAH or MOAH (Biedermann & Grob, 2015;Bordajandi, Dabrio, Ulberth, & Emons, 2008;Chalbot, Vei, Lykoudis, & Kavouras, 2006), HPLCeMS/MS for bisphenols (Gallart-Ayala, Moyano, & Galceran, 2010;P erez-Palacios et al, 2012) and PFC (Begley et al, 2005Poothong et al, 2012;Trier et al, 2011), whereas ink photoinitiators have been analyzed by both techniques (Bugey et al, 2013;Sagratini et al, 2008;Shen, Lian, Ding, Xu, & Shen, 2009). Derivatization procedures were also developed for bisphenols and PFCA to make them amenable for GCeMS (Dufkov a, Cabala, & Sev cík, 2012;Viñas, Campillo, Martínez-Castillo, & Hern andez-C ordoba, 2010).…”

Quantitation and Human Monocyte Cytotoxicity of the Polymerization Agent 1-Hydroxycyclohexyl Phenyl Ketone (Irgacure 184) from Three Brands of Aqueous Injection Solution

“…Shen et al 35) showed that photoinitiators can easily migrate from packaging to foods with a high fat content. The cytotoxicity of compounds like photoinitiators has been thought to be due in part to their hydrophobicity 36) since permeability through the phospholipid bilayer of cellular membranes increases with compound hydrophobicity.…”